HuagongsheHuagongshe Chemistry Print Report · For research reference only
Nitric Acid → HCID 178525367, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Nitric Acid | HCID 944 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Sodium Nitrite | HCID 23668193 | — |
| Reactant | HCID 178471187 | HCID 178471187 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178525367 | HCID 178525367 | 99% |
Reaction Steps
ethyl 3-(5-mercapto-1H-1,2,4-triazol-3-yl)propanoate obtained in Reference Example 21 (650 mg, 3.23 mmol) was added slowly to a mixed solution of sodium nitrite (8.91 mg, 0.129 mmol), nitric acid (3 mL) and water (6 mL) while keeping 45° C. or less. The solution was stirred at room temperature for 15 hr, and neutralized with saturated aqueous sodium carbonate solution. The mixture was concentrated under reduced pressure, and the residue was crystallized from THF, and washed with THF. Ethanol was added thereto, and the insoluble material was filtered off. The filtrate was concentrated under reduced pressure to give the title compound as a pale-yellow powder (454 mg, 99%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07915267B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-a59324fd1b614714b2232481ddd1fe01 |
| Source note | uspto-grants-2011_03 |